Characterization of industrial processed milk by analysis of heat-induced changes

Summary Thermal indicators in milk, which had been subjected to one of the six industrial processes of thermization, pasteurization, direct and indirect UHT-sterilization, pre-sterilization and in-bottle sterilization, were studied. The following three indices of heat damage were analyzed by high performance liquid chromatography (HPLC), hydroxymethylfurfural (HMF), lactulose and acid-soluble β-lactoglobulin(β-LG). Average amounts found were 1710 mg/l of β-LG and 2.49 μmol/l of HMF in pasteurized milk. In UHT milk, the amounts for direct and indirect processes were 389 and 322 mg/l of β-LG, 12.0 and 250 mg/l of lactulose and 5.6 and 8.7 μmol/l of HMF. In sterilized milk the amounts were 1120 mg/l of lactulose and 22 μmol/l of HMF, without any detectable presence of undenatured whey proteins. On the basis of the time/temperature profiles, a sterilization factor, expressed as seconds, was defined for each thermal treatment. By applying discriminant analysis each industrial process could be classified independently at the 95% confidence level (pasteurization, UHT-treatment and in-bottle sterilization), but direct-UHT treated milk could not be discriminated from indirect-UHT milk, nor thermized milk from raw bulk milk. The simultaneous application of several heat-induced parameters improves the classification of industrial processed milks, and is therefore a useful tool for optimization of the processing conditions.     

牛乳中反式脂肪酸在不同热处理条件下的含量变化及热杀菌工艺评价

目的：探讨牛乳中反式脂肪酸(TFA)在不同热处理条件下的变化规律,为工艺参数确立提供依据。方法：采用罗兹-哥特里法提取乳中脂肪,经甲酯化反应后进行气相色谱分析,对牛乳中的TFA含量进行分析比较。结果：在85℃条件下,随着加热时间的延长,牛乳中TFA含量呈显著上升趋势(P＜0.05);相同时间内在超高温(T＞133℃)条件下,提高灭菌温度,牛乳中TFA含量变化不大(P＞0.05);延长灭菌时间,TFA含量明显增加(P＜0.05)。结论：以减少TFA生成量为主要依据确立的巴氏杀菌工艺参数是：85℃、15s;UHT工艺参数为(137±2)℃、4s。     

UHT Milk Processing—Effect on Process Energy Requirements

Energy requirements for processing milk using a free falling film steam infusion ultra-high temperature (UHT) sterilization process and a high temperature-short time (HTST) pasteurization process were determined and compared. Product flow rate was 2500 kg/hr. Milk to milk regeneration was used with both processes. UHT process temperatures were 138, 143, 149, and 154°C. The energy requirements for the UHT and HTST processes ranged between 573 and 667 kJ/kg milk and 217 and 228 kJ/kg milk, respectively. Although the UHT process consumed between 345 and 450 W/kg milk additional energy in the plant, the UHT sterilization of milk has been estimated to result in a net energy savings of 547 - 652 kJ/kg milk because the product does not require post-processing refrigeration.     

Effect of Processing and Storage Conditions on the Fate of Vitamins B1, B2, and C and on the Shelf-Life of Goat's Milk

Goat's milk was heat-processed under different time-temperature conditions of pasteurization and sterilization. Losses of thiamin, riboflavin, and total vitamin C in HTST, Flash, and UHT were less than that by LTLT and Autoclave. Also residual oxygen in the milk affected the loss of total vitamin C during storage. A longer shelf-life of pasteurized milk was obtained with HTST, HTST overpasteurization, and Flash process; however, there was no significant difference between UHT and Autoclave sterilized products. From the above results, HTST pasteurization was considered the best process to preserve milk quality.     

Microwave heat treatment application to pasteurization of human milk

A prototype of microwave pasteurizer has been proposed as an alternative for holder pasteurization (HP) routinely used in Human Milk Bank (HMB), ensuring microbiological safety of human milk (HM). It was shown that the time of heat generation was about 15–16 min shorter by applying the microwave than in HP. Total inactivation of heat-sensitive bacteria Escherichia coli, Pseudomonas aeruginosa, Staphylococcus aureus, and Staphylococcus epidermidis, suspended in milk, occurred in the temperature 62–72 °C in HP. In the case of heat-resistant enterococci the level of inactivation depended on the conditions of the process and the properties of the strains. The application of microwave heating allows to obtain lower D-value than those achieved during HP. The using of microwave heating at 62.5 or 66 °C for 5 or 3 min, respectively, allows to inactivation of HM microbiota. Appropriate microbiological quality of milk is critical for the effectiveness of the pasteurization process.Industrial relevanceLooking for new methods of donor human milk (HM) preservation is dictated by the necessity of providing microbiological safety and, at the same time, maintain its high nutritional and biological value. The holder pasteurization used in the Human Milk Banks (HMB) (heating at 62 °C for 30 min) leads to inactivation of all vegetative forms of microorganisms. Unfortunately, this method causes significant reduction of health benefitting properties of HM. The paper demonstrates the possibility of using the new microwave pasteurizer for preservation of HM, allowing for quick heating of milk to the appropriate temperature and maintaining it in these conditions for a required time. It was shown that the decimal reduction times (D) for strains inoculated to UHT or human milk are several times shorter by using microwave heating than in the commercial pasteurization method. The total inactivation of HM microbiota is obtained after heating at 62.5 and 66 °C for 5 and 3 min, respectively.     

细脚拟青霉深层发酵菌丝体核苷类成分分析

以已知核苷为标样,并以冬虫夏草生药作对比,利用反相高效液相色谱法对细脚拟青霉RCEF0441 深层发酵菌丝体中核苷类化学成分进行分析。结果表明,细脚拟青霉RCEF0441 菌丝体中主要含有胞苷、尿苷、鸟苷、肌苷、胸苷和腺苷6 种核苷,其中胞苷的含量为冬虫夏草生药的3 倍左右,肌苷和鸟苷的含量则分别是冬虫夏草生药的7 和9 倍左右,尿苷和腺苷的含量也显著高于对照品冬虫夏草生药(p<0.05)。     

浸入式和喷射式超高温瞬时灭菌对牛乳中活性蛋白和风味化合物的影响

超高温瞬时灭菌(ultra-high temperature treatment,UHT)是常用的牛乳杀菌技术,可分为直接式与间接式处理,其中直接式UHT技术由于成本高在乳品行业使用较少。近年来,随着消费者对牛乳营养物质和风味需求的升级,直接式UHT技术由于升温速度快、风味及营养成分损失少的优点,再次受到广泛关注。对比了浸入式和喷射式2种直接式处理技术对牛乳理化性质、活性乳清蛋白含量和挥发性化合物含量的影响。结果表明,浸入式UHT乳较喷射式UHT乳的平均粒径、失稳系数和黏度值均更小,但乳清蛋白变性率高。通过2种萃取方法——箭型固相微萃取法和溶剂辅助萃取法,结合气相色谱-质谱联用仪的分析结果,共在UHT乳中检测出59种挥发性化合物,其中,浸入式UHT乳中检测出50种,喷射式UHT乳中检测出52种。浸入式UHT乳中的酮、醛和脂肪酸类化合物比喷射式UHT乳中占比低,而酯类和醇类化合物占比高。主成分分析结果表明,浸入式UHT乳和喷射式UHT乳可根据挥发性化合物进行区分,说明不同的直接式UHT工艺可能对UHT乳风味产生影响。研究结果表明:若生产奶味更重的UHT乳,可选择喷射式UHT;若生产蒸煮味轻、异味少,且贮藏更为稳定的UHT乳,可选择浸入式UHT。研究结果旨在对乳品企业选择恰当的热杀菌工艺,生产货架期长、营养成分高、风味良好的UHT乳提供数据支撑与理论参考。     

Comparison of heat stability of goat milk subjected to ultra-high temperature and in-container sterilization

Goat milk with and without stabilizing salt was subjected to in-container and UHT sterilization. Heat stability was assessed by measuring the amount of sediment in the milk. Without stabilizing salts, goat milk usually produced less sediment when subjected to in-container sterilization compared with UHT processing. Addition of stabilizing salts up to 12.8mM resulted in a progressive increase in sediment for in-container sterilization. In contrast, adding stabilizing salts at 6.4mM initially reduced sediment formation in UHT-treated milk but addition of stabilizing salts at 12.8mM increased sediment formation. Adding stabilizing salts to goat milk increased pH, decreased ionic calcium, and increased ethanol stability. Adding up to 2mM calcium chloride increased sediment formation more after UHT treatment than after in-container sterilization. These results suggest that no single mechanism or set of reactions causes milk to produce sediment during heating and that the favored pathway is different for UHT and in-container sterilization processes. Poor heat stability could be induced both by increasing ionic calcium and by decreasing it. Ethanol stability is not a good indicator of heat stability for in-container sterilization, but it may be for UHT sterilization, if milk does not enter the region of poor heat stability found at low concentrations of ionic calcium.     

不同灭菌工艺对鲜榨柚汁品质及挥发性成分的影响

本文对三种果汁杀菌工艺(热杀菌、UHT杀菌和超高压杀菌)对柚果汁pH、Brix、总酸、维生素C、微生物、感官和香气的影响进行比较。与对照组相比,不同灭菌处理方法对于果汁理化指标并无显著性差异(P<0.05),相对于超高压灭菌,经热杀菌和UHT处理的柚汁的维生素C含量发生显著性降低(P<0.05),这表明超高压处理更利于果汁中维生素C的保存。结合感官评价及GCMS对挥发性成分分析,热处理状态下果汁清香感、柚香感强度出现明显下降,过熟味强度出现明显上升,主要是由于热处理后果汁中醛类、萜烯类成分浓度下降而芳樟醇氧化物浓度增加。该研究结果可为果汁加工提供参考。     

Development and application of a liquid chromatographic method for analysis of nucleotides and nucleosides in milk and infant formulas

A method for the simultaneous determination in milk of the 5′-mononucleotides adenosine 5′-monophosphate, cytidine 5′-monophosphate, guanosine 5′-monophosphate, inosine 5′-monophosphate and uridine 5′-monophosphate and their corresponding nucleosides is described. Following deproteinisation, the sample extract was analysed by reversed-phase liquid chromatography, whereby chromatographic separation was achieved using a polymer grafted silica C₁₈ column, gradient elution with a simple binary mobile phase and UV detection by photodiode array. Performance parameters included recoveries of 95.5–105.2% and precision evaluated as 3.42–6.38% relative standard deviation. The described technique has been applied to the analysis of bovine and human milk, a range of commercial bovine milk-based infant and follow-on formulas, a seasonal study of skim milk powders and an assessment of alkaline phosphatase influence on nucleotide retention.     

D-Amino Acids in Milk as Related to Heat Treatments and Bacterial Activity

The occurrence in milk of free and bound D-amino acids was investigated by chiral phase GC and related to heat treatments and bacterial activity. Significant amounts of free D-alanine (D-Ala), D-aspartic acid (D-Asp), and D-glutamic acid (D-Glu) have been found in raw cow milk but not in human milk. The amount did not increase by pasteurization, UHT treatment, and sterilization. In contrast, the content of D-Ala in raw milk samples increased during cold storage at 4°C, and it was suggested that D-Ala may be considered as an indicator of bacterial milk contamination. The presence of D-Ala, D-Asp and D-Glu detected in milk protein hydrolysates was due to hydrolysis conditions.     

不同杀菌方式对桑葚原汁品质的影响

以桑葚原汁为材料,对比分析了巴氏杀菌、超高温瞬时杀菌（ultra high temperature treated,UHT）以及静态超高压杀菌（ultra high hydrostatic pressure,UHHP）3 种不同的杀菌处理对桑葚原汁的微生物、品质和香气成分的影响。结果表明：3 种杀菌方式处理的桑葚原汁均符合GB 19297-2003《果、蔬汁饮料卫生标准》要求,UHT杀菌更彻底,未有微生物检出。与未杀菌桑葚原汁相比,可溶性固形物、总糖含量经巴氏杀菌和UHT处理后都出现了较显著下降趋势（P＜0.05）;UHHP处理对花色苷含量影响最大;总酚含量、类黄酮含量以及抗氧化能力经过不同杀菌处理后表现出不同程度的下降,UHHP处理影响最小。采用固相微萃取-气相色谱-质谱联用技术对未杀菌桑葚原汁及巴氏杀菌、UHT和UHHP桑葚原汁香气成分进行分析,分别鉴定出52、42、44、49 种挥发性香气成分。UHHP桑葚原汁各主要香气成分与未杀菌桑葚原汁最为接近。UHHP技术不仅具有良好的杀菌效果,而且能较好的保持桑葚原汁的品质。     

Synergistic effects of various lipases and phospholipase C on milk fat

The enzyme, phospholipase C, from a number of psychrotrophs isolated from milk was shown to survive HTST pasteurization and UHT sterilization processes. The phospholipase C of Bacillus cereus was able to increase lipolytic activity of a commercial lipase preparation and native milk lipoprotein lipase in raw milk by making the substrate more susceptible to hydrolysis: phospholipase C had no effect on the lipase activity of a fluorescent Pseudornonas spp. The enhancement of lipolysis by phospholipase C was affected by pronase and papain, but not by trypsin. Homogenization of the raw milk had the same effect on lipolysis by lipoprotein lipase as addition of phospholipase C.     

Heating Milk: A Study on Mutagenicity

The mutagenicity of heated milk and model systems was investigated by the Ames mutagenicity assay. Heating varied from pasteurization to in-bottle sterilization to ultra-high-temperature (UHT) heat-treatment. No mutagenic response was found in heated milk or model systems. Early Maillard reaction products formed in heated milk or milk-resembling model systems apparently did not show mutagenic activity in the Ames-test. Milk that was burnt to the pan was also investigated. Chloroform and ethanol extracts of this milk showed mutagenic activity. Evidence showed this was due to Maillard reaction products. The antimutagenic activity of casein, reported in earlier studies, was confirmed.     

中国巴氏奶 如何再发展

<正> 巴氏奶国外概况巴氏奶(英文称之为 Fresh milk)是巴氏杀菌奶(或巴氏杀菌乳)的简称。是法国微生物学家、化学家巴斯德(louis Pasteur,1822-1895)于1863年在科学实验研究微生物过程中所发明的利用72至76摄氏温度,其受热时间为15秒,利用低温热力将牛奶中的大部分有害微生物(如布氏杆菌、结核杆菌、痢疾杆菌、伤寒杆菌等,但芽孢不能被彻底杀死)杀灭所生产出的一种牛奶产品。这种牛奶处理方法比较温和,在杀灭牛奶中的致病菌而有     

Metabolites of nucleic acids in bovine milk

To investigate metabolites of nucleic acids in milk as by-products of protein biosynthesis, a method for determination of pyrimidine and purine compounds by reversed-phase high-pressure liquid chromatography was developed. Reproducibility of the measured compounds was 2%. Recovery of the main constituents averaged about 99%. In addition to orotic acid, allantoin, and uric acid, the free bases hypoxanthine, xanthine, and guanine, the ribonucleosides uridine, cytidine, and pseudouridine, and the ribonucleotides, guanosine 5'-monophosphate and cytidine 5'-monophosphate, were quantified in milk samples of Holstein-Friesian cows. Milk production from days 45 to 65 of lactation influenced concentrations of individual metabolites differently. Concentrations of orotic acid, allantoin, and uric acid decreased with increasing milk production, whereas concentrations of uridine, cytidine, pseudouridine, hypoxanthine, xanthine, and guanine remained unchanged. The results allowed conclusions on rate limiting steps of catabolic pathways of pyrimidines and purines and indicated relationships with protein biosynthesis. A possible role of metabolites of nucleic acids as taste factors and as substrates for milk microbes is suggested.     

降膜式蒸发器中杀菌的结构优缺点

在奶粉生产中,降＆式蒸发魏有杀菌装置,随着对奶粉质量要求的提高,杀菌的结构形式也发生了变化。目前杀菌的形式主要有间接式杀菌与直接式杀菌两种,根据所用加热介质的不同,间接式杀菌又分为蒸汽间接式杀菌与高温水间接加热杀菌即UHT式杀菌。就不同杀菌结构形式在实际应用中的效果及优缺点进行了阐述。     

Effects of overprocessing on heat damage of UHT milk

Formation of lactulose, furosine, galactosyl-|*beta*|-pyranone and lysinoalanine was studied in UHT milk samples produced by either direct or indirect heating on industrial plants and by indirect heating on a pilot plant. In particular, the effects of severe sterilization conditions, different proportions of milk recirculation, and storage of the finished product (23 °C for up to 90 days) have been investigated on the levels of the above molecules in UHT milk. An extensive increase of the values of all the indicators occurred when severe heat process was applied, but no direct relation was found between their levels and the nominal time–temperature conditions. Lactulose and furosine levels confirmed to be strictly correlated in UHT milk. In case of overheating or high proportion (60%) of milk recirculation, galactosyl-|*beta*|-pyranone formation was strongly enhanced, proving that also the advanced Maillard reaction takes place extensively, which is not detected by furosine value. Formation of lysinoalanine in UHT drinking milk on storage was pointed out for the first time. Lysinoalanine proved to be the most sensitive index of storage conditions among the four parameters studied. Data suggest that a realistic defence of UHT milk quality can be achieved only by fixing upper limits to heat damage parameters. Besides avoiding unjustified milk overheating, this approach may allow manipulations, like reprocessing expired milk, to be pointed out.     

Processing effects on physicochemical properties of creams formulated with modified milk fat

Type of thermal process [high temperature, short time pasteurization (HTST) or ultra-high temperature pasteurization (UHT)] and homogenization sequence (before or after pasteurization) were examined for influence on the physicochemical properties of natural cream (20% milk fat) and creams formulated with 20% low-melt, fractionated butteroil emulsified with skim milk, or buttermilk and butter-derived aqueous phase. Homogenization sequence influenced physicochemical makeup of the creams. Creams homogenized before pasteurization contained more milk fat surface material, higher phospholipid levels, and less protein at the milk fat interface than creams homogenized after pasteurization. Phosphodiesterase I activity was higher (relative to protein on lipid globule surface) when cream was homogenized before pasteurization. Creams formulated with skim milk and modified milk fat had relatively more phospholipid adsorbed at the milk fat interface. Ultra-high-temperature-pasteurized natural and reformulated creams were higher in viscosity at all shear rates investigated compared with HTST-pasteurized creams. High-temperature, short time-pasteurized natural cream was more viscous than HTST-pasteurized reformulated creams at most shear rates investigated. High-temperature, short time-pasteurized creams had better emulsion stability than UHT-pasteurized creams. Cream formulated with buttermilk had creaming stability most comparable to natural cream, and cream formulated with skim milk and modified butteroil was least stable to creaming. Most creams feathered in a pH range of 5.00 to 5.20, indicating that they were moderately stable to slightly unstable emulsions. All processing sequences yielded creams within sensory specifications with the exception of treatments homogenized before UHT pasteurization and skim milk formulations homogenized after UHT pasteurization.     

UHT乳非商业无菌原因分析及质量控制

分析了UHT奶非商业无菌的原因。依据GB/T4789.26-2003和ATD细菌生化鉴定义对UHT奶进行检测及细菌鉴定。结果表明,同一品牌不同品种的6种UHT奶中,有5种为非商业无菌;分别检出蕈状芽孢杆菌短小芽孢杆菌。结论:UHT乳质量把关须从原料乳,生产工艺,生长环境控制。